CN105038586A - Superhydrophobic paint, and preparation method and application thereof - Google Patents
Superhydrophobic paint, and preparation method and application thereof Download PDFInfo
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- CN105038586A CN105038586A CN201510505184.1A CN201510505184A CN105038586A CN 105038586 A CN105038586 A CN 105038586A CN 201510505184 A CN201510505184 A CN 201510505184A CN 105038586 A CN105038586 A CN 105038586A
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- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 285
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003973 paint Substances 0.000 title abstract 9
- -1 polysiloxane Polymers 0.000 claims abstract description 78
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000002904 solvent Substances 0.000 claims abstract description 55
- 238000000926 separation method Methods 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000005191 phase separation Methods 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 22
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 107
- 239000011248 coating agent Substances 0.000 claims description 103
- 239000012528 membrane Substances 0.000 claims description 67
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 44
- 239000000047 product Substances 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 229910001220 stainless steel Inorganic materials 0.000 claims description 34
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 32
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 29
- 239000008096 xylene Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 27
- 229920000742 Cotton Polymers 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 23
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 22
- 239000004677 Nylon Substances 0.000 claims description 13
- 229920001778 nylon Polymers 0.000 claims description 13
- 239000004753 textile Substances 0.000 claims description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002033 PVDF binder Substances 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 229920002301 cellulose acetate Polymers 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 239000002657 fibrous material Substances 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229920002492 poly(sulfone) Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 244000025254 Cannabis sativa Species 0.000 claims description 2
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 2
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 2
- 229920006052 Chinlon® Polymers 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- 229920002334 Spandex Polymers 0.000 claims description 2
- 229920004933 Terylene® Polymers 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 235000009120 camo Nutrition 0.000 claims description 2
- 235000005607 chanvre indien Nutrition 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 238000005187 foaming Methods 0.000 claims description 2
- 239000011487 hemp Substances 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 239000004759 spandex Substances 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 210000002268 wool Anatomy 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 239000011538 cleaning material Substances 0.000 abstract description 2
- 238000003618 dip coating Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 60
- 239000000243 solution Substances 0.000 description 57
- 239000004745 nonwoven fabric Substances 0.000 description 41
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 40
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 40
- 238000012360 testing method Methods 0.000 description 38
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 description 36
- 238000003760 magnetic stirring Methods 0.000 description 35
- 239000007788 liquid Substances 0.000 description 28
- 239000003921 oil Substances 0.000 description 27
- 235000019198 oils Nutrition 0.000 description 27
- 235000019476 oil-water mixture Nutrition 0.000 description 25
- 239000006185 dispersion Substances 0.000 description 21
- 239000011780 sodium chloride Substances 0.000 description 20
- 239000003350 kerosene Substances 0.000 description 18
- 238000004140 cleaning Methods 0.000 description 17
- 239000007864 aqueous solution Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 12
- 238000004132 cross linking Methods 0.000 description 11
- 125000004122 cyclic group Chemical group 0.000 description 10
- 239000007762 w/o emulsion Substances 0.000 description 10
- 239000002585 base Substances 0.000 description 9
- 230000008021 deposition Effects 0.000 description 9
- 239000004814 polyurethane Substances 0.000 description 9
- 229920002635 polyurethane Polymers 0.000 description 9
- 238000009210 therapy by ultrasound Methods 0.000 description 9
- 238000002791 soaking Methods 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 4
- 244000137852 Petrea volubilis Species 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000010494 opalescence Effects 0.000 description 3
- 150000001447 alkali salts Chemical class 0.000 description 2
- 239000008157 edible vegetable oil Substances 0.000 description 2
- 239000003759 ester based solvent Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000295 fuel oil Substances 0.000 description 2
- 230000005251 gamma ray Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000005453 ketone based solvent Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a superhydrophobic paint, and a preparation method and application thereof. The preparation method of the micro/nano superhydrophobic paint comprises the following steps: 1) dissolving fluorinated polysiloxane in a solvent a to obtain a solution a; 2) dropwisely adding a solvent b into the solution a obtained in the step 1) to perform phase separation, wherein the obtained system is the micro/nano superhydrophobic paint; and centrifuging the micro/nano superhydrophobic paint to obtain the nano superhydrophobic paint. After the two paints are applied onto various substrates by dip coating or spray coating, the substrates can be superhydrophobic; and the paint can be used for self-cleaning materials, waterproof materials, oil-water separation materials and the like. Besides, the superhydrophobic material prepared from the paint has the characteristics of solvent resistance, acid/alkali resistance, friction resistance, high temperature resistance (up to 400 DEG C) and the like.
Description
Technical Field
The invention belongs to the field of coatings, and relates to a super-hydrophobic coating, and a preparation method and application thereof.
Background
The super-hydrophobic is a phenomenon that the static contact angle of water drops on the surface of an object is more than 150 degrees, and the rolling angle is less than 10 degrees. Two conditions are generally satisfied for constructing a superhydrophobic surface: micro-nano multilevel structure and low surface energy. In recent years, superhydrophobic surfaces have been widely used in the fields of self-cleaning, waterproofing, oil-water separation, and the like. However, most of the super-hydrophobic materials are complex in preparation process, and the microstructure on the surface of the material is extremely easy to damage, so that the super-hydrophobicity is difficult to maintain in the using process.
Disclosure of Invention
The invention aims to provide a super-hydrophobic coating and a preparation method and application thereof.
The invention provides a method for preparing a micro-nano super-hydrophobic coating, which comprises the following steps:
1) dissolving fluorinated polysiloxane in a solvent a to obtain a solution a;
2) adding a solvent b into the solution a obtained in the step 1) in a dropwise manner for phase separation to obtain a system, namely the micro-nano super-hydrophobic coating;
the solvent a is at least one of a few ketone solvent and an ester solvent such as tetrahydrofuran, acetone, ethyl acetate, butanone and the like;
the solvent b is at least one selected from alcohols or hydrocarbon solvents such as methanol, ethanol, isopropanol, water, toluene, xylene, n-hexane and cyclohexane; solvent b is a non-solvent for the fluorinated polysiloxane.
In the above method, the fluorinated polysiloxane is a polysiloxane having a fluorine atom in a side chain thereof, and specifically is at least one selected from the group consisting of polytrifluoropropylmethylsiloxane (PTFPMS), Polymethylnonafluorohexylsiloxane (PNFHMS), Polytridecylfluorooctylmethylsiloxane (PTDFOMS), and Polymethylheptadecafluorodecylsiloxane (PHDFDMS);
wherein the weight average molecular weight of the polytrifluoropropylmethylsiloxane (PTFPMS) is 3000-100 ten thousand, specifically 5000-5 ten thousand, and more specifically 1 ten thousand;
the weight average molecular weight of the poly (methyl nonafluorohexylsiloxane) (PNFHMS) is 4000-200 ten thousand, specifically 5000-5 ten thousand, more specifically 2 ten thousand;
the weight average molecular weight of the Polytridecylfluorooctylmethylsiloxane (PTDFOMS) is 5000-250 ten thousand;
the weight-average molecular weight of the Polymethylheptadecafluorodecylsiloxane (PHDFDMS) is 6000-300 ten thousand;
in the solution a, the concentration of the fluorinated polysiloxane is 0.1-200mg/ml, preferably 25-50 mg/ml;
the mass ratio of the fluorinated polysiloxane to the solvent b is 1: 10-10000, preferably 1: 20-600.
In the step 1), the dissolving mode is stirring and dissolving; the stirring speed is 100-3000rpm, specifically 800-1000 rpm; stirring for 1-30 days, specifically 5 days;
in the step 2), the dripping speed is 1 drop per second to 1 second and 10 drops per second;
the phase separation mode is stirring; the stirring speed is 100-3000rpm, specifically 500-1000rpm, more specifically 500rpm, 700rpm, 900rpm, 1000 rpm.
In addition, the micro-nano super-hydrophobic coating prepared by the method also belongs to the protection scope of the invention. Wherein, in the micro-nano super-hydrophobic coating, the particle size of the aggregate is 20 nm-20 μm. The aggregate is in particular a fluorinated polysiloxane aggregate.
The invention also provides a method for preparing the nanoscale superhydrophobic coating, which comprises the following steps: centrifuging the micro-nano super-hydrophobic coating provided by the invention, and collecting supernatant obtained after centrifugation to obtain the nano super-hydrophobic coating.
In the centrifugation step of the method, the centrifugation rotating speed is 500rpm-12000rpm, the centrifugation time is 5min-30min, and the centrifugation radius is 6-12 cm.
In addition, the nano-scale super-hydrophobic coating prepared by the method also belongs to the protection scope of the invention.
In the nanoscale superhydrophobic coating, the particle size of the aggregate is 20nm-100 nm. The aggregate is in particular a fluorinated polysiloxane aggregate; the nanoscale superhydrophobic coating exhibits bluish opalescence.
The invention also provides application of the super-hydrophobic coating.
Specifically, the application of the micro-nano super-hydrophobic coating or the nano super-hydrophobic coating in preparing a super-hydrophobic product, the application of the nano super-hydrophobic coating in preparing a super-hydrophobic filter membrane, or the super-hydrophobic product prepared from the micro-nano super-hydrophobic coating or the nano super-hydrophobic coating, or the super-hydrophobic filter membrane prepared from the nano super-hydrophobic coating also belong to the protection scope of the invention.
Wherein the pore diameter of the super-hydrophobic product is 1-1000 μm;
the aperture of the super-hydrophobic filter membrane is 20nm-900nm, and specifically can be 220nm-450 nm.
The invention provides a method for preparing a super-hydrophobic product, which comprises the following steps:
and (3) dipping or spraying the micro-nano super-hydrophobic coating provided by the invention on a substrate, and drying to obtain the super-hydrophobic product.
In the method, the material for forming the substrate is fiber or porous material, specifically fabric, sponge, metal filter screen or filter paper; the fabric is a natural textile or an artificial textile, and the natural textile is a cotton, hemp, silk or wool textile; the artificial textile is a terylene, polypropylene, chinlon, spandex or acrylic textile; the sponge is polyester, polyvinyl alcohol foaming sponge or polyether sponge; the metal filter screen is a stainless steel screen with the average aperture of 30-1000 μm; the filter paper is qualitative filter paper or quantitative filter paper;
in the drying step, the temperature is 25-100 ℃, and the time is 1-24 h, specifically 2h or 3 h.
The method for preparing the super-hydrophobic filter membrane comprises the following steps:
and (3) coating the nanoscale superhydrophobic coating on a filter membrane under a vacuum condition, and drying to obtain the superhydrophobic filter membrane.
In the method, the aperture of the filter membrane is 20nm-900nm, specifically 220nm-450 nm;
the filter membrane is a nylon membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane, a mixed fiber ester membrane, a glass fiber membrane, an aluminum oxide membrane, a polyamide membrane, a cellulose acetate membrane, a polysulfone membrane, a polyether sulfone membrane or a polyvinyl alcohol membrane;
in the vacuum condition, the vacuum degree is 0.02-0.1 MPa;
in the drying step, the temperature is 30-100 ℃, and the time is 1-24 h, specifically 2h or 3 h.
In addition, the super-hydrophobic product or the super-hydrophobic filter membrane prepared by the method and the application of the super-hydrophobic product or the super-hydrophobic filter membrane in oil-water separation also belong to the protection scope of the invention. Wherein the superhydrophobic article is a superhydrophobic article having at least one of the following properties: solvent resistance, acid and alkali resistance, high temperature resistance and mechanical friction resistance;
wherein the high temperature resistance is the highest temperature resistance of 400 ℃.
The oil-water separation specifically comprises the following steps:
1) the oil-water mixture with a certain volume ratio is poured into a separation device which clamps a super-hydrophobic substrate, under the action of gravity, oil passes through the super-hydrophobic substrate, and water is trapped on the substrate, so that the separation of the oil-water mixture is realized.
2) The high-temperature oil-water mixture with a certain volume ratio is poured into a separation device fixed with a super-hydrophobic substrate, under the action of gravity, oil passes through the super-hydrophobic substrate, and water is trapped on the substrate, so that the separation of the high-temperature oil-water mixture is realized.
3) Pouring the water-in-oil emulsion into a separation device, clamping a super-hydrophobic filter membrane by the separation device, and allowing the oil phase in the emulsion to pass through the filter membrane under a certain vacuum pressure to obtain clear filtrate, thereby realizing the separation of the water-in-oil emulsion.
The oil in the step 1) is common organic solvent immiscible with water, fuel oil, edible oil and the like. The volume ratio of the oil-water mixture is not limited.
The super-hydrophobic substrate in the step 1) is made of fiber or porous material, and specifically can be fabric, sponge, metal filter screen, filter paper and the like.
The temperature of the high-temperature oil-water mixture in the step 2) is 90-100 ℃.
The water-in-oil emulsion in the step 3) comprises a surfactant-stabilized water-in-oil emulsion and a surfactant-free water-in-oil emulsion. The oil is common organic solvent, fuel oil, edible oil and the like which are not mutually soluble with water.
The nano-porous filter membrane in the step 3) comprises a nylon membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane, a mixed fiber ester membrane, a glass fiber membrane, an aluminum oxide membrane, a polyamide membrane, a cellulose acetate membrane, a polysulfone membrane, a polyether sulfone membrane, a polyvinyl alcohol membrane and the like with the aperture of 20-900 nm.
The solvent resistance specifically refers to that the super-hydrophobic product prepared from the micro-nano super-hydrophobic coating provided by the invention is subjected to treatment at room temperature60Co is used as a light source, irradiation crosslinking is carried out for 10min by gamma ray irradiation of 100kGy, the contact angle of the crosslinked super-hydrophobic product to water is more than 150 degrees after testing, and the super-hydrophobic product still keeps super-hydrophobicity after being soaked in ketone or ester solvents such as tetrahydrofuran, acetone, ethyl acetate and the like.
The acid and alkali resistance specifically means that acid, alkali and salt aqueous solutions with certain pH values are respectively dripped on the surface of the super-hydrophobic product prepared from the micro-nano super-hydrophobic coating provided by the invention, the acid, alkali and salt liquid drops can easily slide off the surface of the super-hydrophobic product, and the super-hydrophobic product has the characteristics of acid and alkali resistance when the contact angles of the super-hydrophobic product to the acid, the alkali and the salt are all larger than 150 degrees. The pH of the aqueous solution of the acid, the base and the salt is 1 to 14, specifically hydrochloric acid having a pH of 1, sodium hydroxide having a pH of 14 and an aqueous solution of sodium chloride having a pH of 7.
The high temperature resistance specifically means that an inorganic or metal super-hydrophobic product prepared from the micro-nano super-hydrophobic coating provided by the invention is placed in a muffle furnace (below 400 ℃) to be calcined for 1-5 hours, and the contact angle of the calcined product to water is more than 150 degrees, so that the product has the characteristic of high temperature resistance.
The mechanical friction resistance is characterized in that a weight with a certain weight is placed on a super-hydrophobic product prepared from the micro-nano super-hydrophobic coating, and after the super-hydrophobic product is circularly rubbed on the surface of sand paper for a plurality of times within a certain distance, through a test, the contact angle of the rubbed product to water is more than 150 degrees, and the product has the characteristic of mechanical friction resistance. Wherein the weight of the load can be 100-250 g, the number of the friction cycles is 10-100, and the friction distance is 10-30 cm.
The invention has the outstanding advantages that:
1. the preparation method of the micro-nano super-hydrophobic coating and the nano super-hydrophobic coating is simple, and the micro-nano super-hydrophobic coating and the nano super-hydrophobic coating can be prepared only by adding a non-solvent at normal temperature.
2. The preparation method of the super-hydrophobic product is simple and convenient, and the substrate can have super-hydrophobic property only by dip-coating and spraying the dispersion liquid A on the substrate or coating the nano-scale super-hydrophobic coating on the porous filter membrane under certain vacuum pressure and then volatilizing the solvent at normal temperature.
3. The method has universality, and the two types of super-hydrophobic coatings can be coated on a substrate made of any material to endow the substrate with super-hydrophobic characteristics.
4. The super-hydrophobic material modified by the two super-hydrophobic coatings has the characteristics of acid and alkali resistance, solvent resistance, mechanical friction resistance, high temperature resistance (up to 400 ℃) and the like.
5. The substrate modified by the two super-hydrophobic coatings can be used as a self-cleaning material, a waterproof material, an oil-water separation material and the like; in addition, the super-hydrophobic product prepared by the coating also has the characteristics of solvent resistance, acid and alkali resistance, mechanical friction resistance, high temperature resistance (up to 400 ℃) and the like.
Drawings
FIG. 1 is a scanning electron micrograph of the superhydrophobic gauze prepared in example 1, at 330-fold magnification.
FIG. 2 is a graph showing the results of separating an oil-water mixture using the superhydrophobic gauze of example 1.
FIG. 3 is a photograph and an optical microscope photograph of a water-in-oil emulsion before and after separation.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
1) Dissolving 2.5g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone solvent a, and magnetically stirring for 5 days at normal temperature and the rotating speed of 1000rpm to obtain polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely solution a;
2) under the magnetic stirring of 500rpm, 50ml of solvent b deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second, and phase separation is initiated through a non-solvent to obtain a system, namely the dispersion liquid containing the polytrifluoropropylmethylsiloxane (PTFPMS) micro-nano aggregates, namely the micro-nano super-hydrophobic coating.
Soaking pure cotton gauze as a substrate in the micro-nano super-hydrophobic coating for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic gauze.
FIG. 1 is a scanning electron micrograph of the superhydrophobic gauze prepared in this example, at 330 times magnification.
Through tests, the water contact angle of the super-hydrophobic gauze is larger than 150 degrees, the contact angle of the super-hydrophobic gauze to oil (kerosene, normal hexane, xylene, hexadecane and the like) is 0 degree, the super-hydrophobic gauze can be used for separating a macroscopic oil-water mixture, and the separation efficiency exceeds 98 percent, as shown in figures 2 and 3. The super-hydrophobic gauze can also be used for self-cleaning products, waterproof materials and the like.
Subjecting the super-hydrophobic gauze to room-temperature atmospheric environment60Co is used as a light source, irradiation crosslinking is carried out for 10min by gamma ray irradiation of 100kGy, after treatment and test, the contact angle of the gauze to water is still larger than 150 degrees, and the super-hydrophobicity can still be maintained after the gauze is soaked in ketone or ester solvents such as tetrahydrofuran, acetone, ethyl acetate and the like.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic gauze, the drops can easily slide off the surface, and the contact angles of the gauze to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7 are all more than 150 degrees and have the characteristic of acid-base salt resistance.
A weight of 150g is placed on the super-hydrophobic gauze, and after the super-hydrophobic gauze is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic gauze to water is more than 150 degrees through testing, and the super-hydrophobic gauze has the characteristic of mechanical friction resistance.
Example 2
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is the dispersion liquid containing the micro-nano aggregates, namely the micro-nano super-hydrophobic coating.
And (3) immersing the polypropylene non-woven fabric into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic non-woven fabric. Tests show that the super-hydrophobic non-woven fabric has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating a macroscopic oil-water mixture, and has separation efficiency of more than 98 percent. The super-hydrophobic non-woven fabric can also be used as a self-cleaning product, a waterproof material and the like.
Example 3
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
The polyurethane sponge is immersed into the micro-nano super-hydrophobic coating for deposition for 3-5min, the coating is taken out and dried for 2h at normal temperature, and the super-hydrophobic sponge is obtained after the solvent is volatilized, and tests show that the super-hydrophobic sponge has a contact angle of more than 150 degrees to water and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has the separation efficiency of more than 98%. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Example 4
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone, and stirring for 5 days at normal temperature under the magnetic stirring of 800rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 900rpm, 100ml of deionized water is added into the solution a obtained in the step 1) drop by drop for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
And (3) putting the absorbent cotton into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out, drying at normal temperature for 3h, and volatilizing the solvent to obtain the super-hydrophobic absorbent cotton. Tests show that the super-hydrophobic absorbent cotton has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating macroscopic oil-water mixtures, and has a separation efficiency of more than 98 percent. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Example 5
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone, and stirring for 5 days at normal temperature under the magnetic stirring of 900rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 700rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
And (3) filling the micro-nano super-hydrophobic coating into a spray can, spraying the micro-nano super-hydrophobic coating on the surface of a stainless steel wire mesh, wherein the average pore diameter of the stainless steel wire mesh is less than 200 mu m, drying for 2h at normal temperature after spraying for a plurality of times, and volatilizing a solvent to obtain the super-hydrophobic stainless steel wire mesh. Through tests, the contact angle of the super-hydrophobic stainless steel wire mesh to water is larger than 150 degrees, the contact angle to oil is 0 degree, and the super-hydrophobic stainless steel wire mesh can be used for separating a macroscopic oil-water mixture. The separation efficiency is over 98 percent. The super-hydrophobic stainless steel wire mesh can also be used as a self-cleaning product, a waterproof material and the like. Due to the high-temperature resistance of the super-hydrophobic coating, the super-hydrophobic stainless steel wire mesh can be used for separating high-temperature (90-100 ℃) oil-water mixtures.
The super-hydrophobic stainless steel wire mesh is placed in a muffle furnace and calcined for 2 hours at 400 ℃, and through testing, the contact angle of the calcined stainless steel wire mesh to water is larger than 150 degrees, and the super-hydrophobic stainless steel wire mesh has the characteristic of high temperature resistance.
Example 6
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of acetone, and stirring for 5 days at normal temperature under the magnetic stirring of 900rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 900rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
Centrifuging the micro-nano super-hydrophobic coating for 10min at the rotating speed of 12000rpm to obtain a dispersion liquid B only containing nano aggregates and having blue opalescence, namely the nano super-hydrophobic coating, wherein the particle size of the aggregates in the nano super-hydrophobic coating is 20 nm.
The nano-scale super-hydrophobic coating is coated on the surface and the interior of a 450nm nylon membrane under the vacuum pressure of 0.04MPa, the nylon membrane is placed in an oven at 80 ℃ and dried for 3 hours, and after testing, the water contact angle of the modified nylon membrane in air is 120 degrees, the contact angle to oil (kerosene, n-hexane, xylene, hexadecane and the like) is 0 degree, the contact angle to water in oil (kerosene, n-hexane, xylene, hexadecane and the like) phase is more than 150 degrees, the contact angle to oil is 0 degree, the nylon membrane can be used for separating water-in-oil emulsion without surfactant and with stable surfactant, and the separation efficiency is more than 99.99 percent. Due to the high temperature resistance of the coating, the modified nylon membrane can also be used for separating high-temperature water-in-oil emulsion (90-100 ℃), and the separation efficiency is over 99.99%.
Example 7
1) Dissolving 2.5g of trifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a trifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 50ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second, and phase separation is carried out through non-solvent initiation, so that the obtained system is the dispersion liquid containing the trifluoropropylmethylsiloxane (PTFPMS) micro-nano-sized aggregates, namely the micro-nano super-hydrophobic coating.
Soaking pure cotton gauze as a substrate in the micro-nano super-hydrophobic coating for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic gauze. Tests show that the super-hydrophobic gauze has a water contact angle of more than 150 degrees and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has a separation efficiency of more than 98 percent. The super-hydrophobic gauze can also be used for self-cleaning products, waterproof materials and the like.
Example 8
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 100ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is a dispersion liquid simultaneously containing micro-nano aggregates, namely the micro-nano super-hydrophobic coating.
Immersing the polypropylene non-woven fabric into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out the non-woven fabric, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic non-woven fabric. Tests show that the super-hydrophobic non-woven fabric has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating a macroscopic oil-water mixture, and has separation efficiency of more than 98 percent. The super-hydrophobic non-woven fabric can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting the super-hydrophobic non-woven fabric to vacuum filtration at room temperature under atmospheric environment60Irradiating the surface of the non-woven fabric for 10min by 100kGy gamma rays with Co as a light source, performing surface irradiation crosslinking, sequentially putting the non-woven fabric into ethanol, n-hexane and xylene, performing ultrasonic treatment for 20h, taking out the non-woven fabric, drying, and testing to obtain the non-woven fabric with a contact angle of more than 150 degrees to water and solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic non-woven fabric, the liquid drops easily slide off the surface, and the non-woven fabric has the contact angle of more than 150 degrees and has the characteristics of acid and alkali salt resistance to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride liquid drops with pH value of 7.
The super-hydrophobic non-woven fabric is placed with a weight of 150g, and after the super-hydrophobic non-woven fabric is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic non-woven fabric to water is more than 150 degrees through testing, and the super-hydrophobic non-woven fabric has the characteristic of mechanical friction resistance.
Example 9
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under the magnetic stirring of 500rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 1000rpm, 100ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
And (3) immersing the polyurethane sponge into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out the polyurethane sponge, drying the polyurethane sponge for 2h at normal temperature, and volatilizing the solvent to obtain the super-hydrophobic sponge. Tests show that the super-hydrophobic sponge has a contact angle of more than 150 degrees to water and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has a separation efficiency of more than 98 percent. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting the super-hydrophobic sponge to room temperature atmosphere60Irradiating the surface of the sponge by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the sponge into ethanol, n-hexane and xylene for 20h for ultrasonic treatment, taking out the sponge and drying the sponge, wherein the contact angle of the sponge to water is still larger than 150 degrees through a test, and the sponge has the characteristic of solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic sponge, the drops can easily slide off the surface, and the sponge has the contact angle of more than 150 degrees and has the characteristic of acid-base salt resistance to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7.
A weight of 150g is placed on the super-hydrophobic sponge, and after the super-hydrophobic sponge is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic sponge to water is more than 150 degrees, and the super-hydrophobic sponge has the characteristic of mechanical friction resistance.
Example 10
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under the magnetic stirring of 800rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 900rpm, 100ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
And (2) putting absorbent cotton into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out the absorbent cotton, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic absorbent cotton. Tests show that the super-hydrophobic absorbent cotton has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating macroscopic oil-water mixtures, and has a separation efficiency of more than 98 percent. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting super-hydrophobic absorbent cotton to room temperature atmospheric environment60Irradiating the surface of the absorbent cotton by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the absorbent cotton into ethanol, n-hexane and xylene for 20h by ultrasonic treatment, taking out the absorbent cotton and drying the absorbent cotton, and testing to obtain the absorbent cotton with a contact angle of more than 150 degrees to water and solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dripped on the surface of the super-hydrophobic absorbent cotton, the liquid drops easily slide off the surface, and the contact angles of the absorbent cotton to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride liquid drops with pH value of 7 are all larger than 150 degrees and have the characteristic of acid-base salt resistance.
The super-hydrophobic absorbent cotton is placed with a weight of 150g, and after the super-hydrophobic absorbent cotton is subjected to cyclic friction on the surface of sand paper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic absorbent cotton to water is more than 150 degrees, and the super-hydrophobic absorbent cotton has the characteristic of mechanical friction resistance.
Example 11
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under magnetic stirring at 900rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 700rpm, 100ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
Filling the micro-nano super-hydrophobic coating into a bottle with a nozzle, spraying the coating on the surface of a stainless steel wire mesh, wherein the average pore diameter of the stainless steel wire mesh is less than 200 mu m, drying for 2h at normal temperature after spraying for a plurality of times, and volatilizing a solvent to obtain the super-hydrophobic stainless steel wire mesh. Through tests, the contact angle of the super-hydrophobic stainless steel wire mesh to water is larger than 150 degrees, the contact angle to oil is 0 degree, and the super-hydrophobic stainless steel wire mesh can be used for separating a macroscopic oil-water mixture. The separation efficiency is over 98 percent. The super-hydrophobic stainless steel wire mesh can also be used as a self-cleaning product, a waterproof material and the like. Due to the high-temperature resistance of the super-hydrophobic coating, the super-hydrophobic stainless steel wire mesh can be used for separating high-temperature (90-100 ℃) oil-water mixtures.
Subjecting a super-hydrophobic stainless steel wire mesh to room-temperature atmospheric environment60Irradiating the surface of the stainless steel wire mesh by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the stainless steel wire mesh into ethanol, n-hexane and xylene for 20h by ultrasonic treatment, taking out the stainless steel wire mesh and drying the stainless steel wire mesh, wherein the contact angle of the stainless steel wire mesh to water is still larger than 150 degrees through testing, and the stainless steel wire mesh has the characteristic of solvent resistance.
The contact angles of hydrochloric acid with pH value of 1, sodium hydroxide with pH value of 14 and sodium chloride aqueous solution with pH value of 7 on the surface of the super-hydrophobic stainless steel screen are tested to be more than 150 degrees and have the characteristics of acid-base salt resistance.
A weight of 150g is placed on the super-hydrophobic stainless steel wire mesh, and after the stainless steel wire mesh is subjected to cyclic friction on the surface of sand paper (600 meshes) for 40 times within a distance of 15cm, through a test, the contact angle of the stainless steel wire mesh to water is larger than 150 degrees, and the stainless steel wire mesh has the characteristic of mechanical friction resistance.
The super-hydrophobic stainless steel wire mesh is placed in a muffle furnace and calcined for 2 hours at 400 ℃, and through testing, the contact angle of the calcined stainless steel wire mesh to water is larger than 150 degrees, and the super-hydrophobic stainless steel wire mesh has the characteristic of high temperature resistance.
Example 12
1) Dissolving 5.0g of polytrifluoropropylmethylsiloxane (PTFPMS) with the weight-average molecular weight of 1 ten thousand in 100ml of ethyl acetate, and stirring for 5 days at normal temperature under magnetic stirring at 900rpm to obtain a polytrifluoropropylmethylsiloxane (PTFPMS) solution, namely a solution a;
2) under the magnetic stirring of 900rpm, 100ml of ethanol is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
Centrifuging the micro-nano super-hydrophobic coating for 10min at the rotating speed of 12000rpm to obtain a dispersion liquid B only containing nano aggregates and having blue opalescence, namely the nano super-hydrophobic coating, wherein the particle size of the aggregates in the nano super-hydrophobic coating is 20 nm.
The nano-scale super-hydrophobic coating is coated on the surface and the interior of a 450nm nylon membrane under the vacuum pressure of 0.04MPa, the nylon membrane is placed in an oven at the temperature of 80 ℃ to be dried for 2 hours, and after testing, the water contact angle of the modified nylon membrane in the air is 120 degrees, the contact angle to oil (kerosene, n-hexane, xylene, hexadecane and the like) is 0 degree, the contact angle to water in oil (kerosene, n-hexane, xylene, hexadecane and the like) phase is more than 150 degrees, the contact angle to oil is 0 degree, the nylon membrane can be used for separating water-in-oil emulsion without surfactant and stable surfactant, and the separation efficiency is more than 99.99 percent. Due to the high temperature resistance of the coating, the modified nylon membrane can also be used for separating high-temperature water-in-oil emulsion (90-100 ℃), and the separation efficiency is over 99.99%.
Example 13
1) Dissolving 2.5g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 50ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second, and phase separation is carried out through non-solvent initiation, so that the obtained system is the dispersion liquid containing the Polymethylnonafluorohexylsiloxane (PNFHMS) micro-nano-sized aggregates, namely the micro-nano super-hydrophobic coating.
Soaking pure cotton gauze as a substrate in the micro-nano super-hydrophobic coating for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic gauze. Tests show that the super-hydrophobic gauze has a water contact angle of more than 150 degrees and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has a separation efficiency of more than 98 percent. The super-hydrophobic gauze can also be used for self-cleaning products, waterproof materials and the like.
Subjecting the super-hydrophobic gauze to room-temperature atmospheric environment60Irradiating the surface of the gauze by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the gauze into ethanol, n-hexane and xylene for 20h of ultrasonic treatment, taking out the gauze, drying the gauze, and testing to ensure that the contact angle of the gauze to water is still more than 150 degrees and the gauze has the characteristic of solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic gauze, the drops can easily slide off the surface, and the contact angles of the gauze to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7 are all more than 150 degrees and have the characteristic of acid-base salt resistance.
A weight of 150g is placed on the super-hydrophobic gauze, and after the super-hydrophobic gauze is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic gauze to water is more than 150 degrees through testing, and the super-hydrophobic gauze has the characteristic of mechanical friction resistance.
Example 14
1) Dissolving 5.0g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is the dispersion liquid containing the micro-nano aggregates, namely the micro-nano super-hydrophobic coating.
Immersing the polypropylene non-woven fabric into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out the non-woven fabric, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic non-woven fabric. Tests show that the super-hydrophobic non-woven fabric has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating a macroscopic oil-water mixture, and has separation efficiency of more than 98 percent. The super-hydrophobic non-woven fabric can also be used as a self-cleaning product, a waterproof material and the like.
Example 15
1) Dissolving 5.0g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 500rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 1000rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
And (2) soaking the polyurethane sponge into the micro-nano super-hydrophobic coating for deposition for 3-5min, wherein the average pore diameter of the polyurethane sponge is less than 800 microns, taking out the polyurethane sponge, drying the polyurethane sponge for 2h at normal temperature, volatilizing a solvent to obtain the super-hydrophobic sponge, and testing the super-hydrophobic sponge to obtain the super-hydrophobic sponge, wherein the contact angle of the super-hydrophobic sponge to water is more than 150 degrees, the contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) is 0 degree, the super-hydrophobic sponge can be used for separating a macroscopic oil-water mixture, and the. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting the super-hydrophobic sponge to room temperature atmosphere60Irradiating the surface of the sponge by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the sponge into ethanol, n-hexane and xylene for 20h for ultrasonic treatment, taking out the sponge and drying the sponge, wherein the contact angle of the sponge to water is still larger than 150 degrees through a test, and the sponge has the characteristic of solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic sponge, the drops can easily slide off the surface, and the sponge has the contact angle of more than 150 degrees and has the characteristic of acid-base salt resistance to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7.
A weight of 150g is placed on the super-hydrophobic sponge, and after the super-hydrophobic sponge is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic sponge to water is more than 150 degrees, and the super-hydrophobic sponge has the characteristic of mechanical friction resistance.
Example 16
1) Dissolving 2.5g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 50ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second, and phase separation is carried out through non-solvent initiation, so that the obtained system is the dispersion liquid containing the Polymethylnonafluorohexylsiloxane (PNFHMS) micro-nano-sized aggregates, namely the micro-nano super-hydrophobic coating.
Soaking pure cotton gauze as a substrate in the micro-nano super-hydrophobic coating for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic gauze. Tests show that the super-hydrophobic gauze has a water contact angle of more than 150 degrees and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has a separation efficiency of more than 98 percent. The super-hydrophobic gauze can also be used for self-cleaning products, waterproof materials and the like.
Subjecting the super-hydrophobic gauze to room-temperature atmospheric environment60Irradiating the surface of the gauze by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the gauze into ethanol, n-hexane and xylene for 20h of ultrasonic treatment, taking out the gauze, drying the gauze, and testing to ensure that the contact angle of the gauze to water is still more than 150 degrees and the gauze has the characteristic of solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic gauze, the drops can easily slide off the surface, and the contact angles of the gauze to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7 are all more than 150 degrees and have the characteristic of acid-base salt resistance.
A weight of 150g is placed on the super-hydrophobic gauze, and after the super-hydrophobic gauze is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic gauze to water is more than 150 degrees through testing, and the super-hydrophobic gauze has the characteristic of mechanical friction resistance.
Example 17
1) Dissolving 5.0g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 1000rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 500rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is the dispersion liquid containing the micro-nano aggregates, namely the micro-nano super-hydrophobic coating.
Immersing the polypropylene non-woven fabric into the micro-nano super-hydrophobic coating for deposition for 3-5min, taking out the non-woven fabric, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic non-woven fabric. Tests show that the super-hydrophobic non-woven fabric has a contact angle to water of more than 150 degrees and a contact angle to oil (kerosene, normal hexane, xylene, hexadecane and the like) of 0 degree, can be used for separating a macroscopic oil-water mixture, and has separation efficiency of more than 98 percent. The super-hydrophobic non-woven fabric can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting the super-hydrophobic non-woven fabric to vacuum filtration at room temperature under atmospheric environment60Irradiating the surface of the non-woven fabric for 10min by 100kGy gamma rays with Co as a light source, performing surface irradiation crosslinking, sequentially putting the non-woven fabric into ethanol, n-hexane and xylene, performing ultrasonic treatment for 20h, taking out the non-woven fabric, drying, and testing to obtain the non-woven fabric with a contact angle of more than 150 degrees to water and solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic non-woven fabric, the liquid drops easily slide off the surface, and the non-woven fabric has the contact angle of more than 150 degrees and has the characteristics of acid and alkali salt resistance to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride liquid drops with pH value of 7.
The super-hydrophobic non-woven fabric is placed with a weight of 150g, and after the super-hydrophobic non-woven fabric is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic non-woven fabric to water is more than 150 degrees through testing, and the super-hydrophobic non-woven fabric has the characteristic of mechanical friction resistance.
Example 18
1) Dissolving 5.0g of Polymethylnonafluorohexylsiloxane (PNFHMS) with the weight-average molecular weight of 2 ten thousand in 100ml of tetrahydrofuran, and stirring for 5 days at normal temperature under the magnetic stirring of 500rpm to obtain a Polymethylnonafluorohexylsiloxane (PNFHMS) solution, namely a solution a;
2) under the magnetic stirring of 1000rpm, 100ml of deionized water is added dropwise into the solution a obtained in the step 1) at the speed of 1 drop per second for phase separation, and the obtained system is dispersion liquid containing micron-nanometer aggregates, namely the micro-nanometer super-hydrophobic coating.
Soaking polyurethane sponge into the micro-nano super-hydrophobic coating for 3-5min, taking out, drying at normal temperature for 2h, and volatilizing the solvent to obtain the super-hydrophobic sponge. Tests show that the super-hydrophobic sponge has a contact angle of more than 150 degrees to water and a contact angle of 0 degree to oil (kerosene, normal hexane, xylene, hexadecane and the like), can be used for separating a macroscopic oil-water mixture, and has a separation efficiency of more than 98 percent. The super-hydrophobic sponge can also be used as a self-cleaning product, a waterproof material and the like.
Subjecting the super-hydrophobic sponge to room temperature atmosphere60Irradiating the surface of the sponge by 100kGy gamma rays with Co as a light source for 10min for surface irradiation crosslinking, sequentially putting the sponge into tetrahydrofuran, acetone, ethyl acetate, ethanol, n-hexane and xylene for ultrasonic treatment for 20h, taking out the sponge and drying the sponge, wherein the contact angle of the sponge to water is still larger than 150 degrees through testing, and the sponge has the characteristic of solvent resistance.
The hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride aqueous solution with pH value of 7 are dropped on the surface of the super-hydrophobic sponge, the drops can easily slide off the surface, and the sponge has the contact angle of more than 150 degrees and has the characteristic of acid-base salt resistance to the hydrochloric acid with pH value of 1, the sodium hydroxide with pH value of 14 and the sodium chloride drops with pH value of 7.
A weight of 150g is placed on the super-hydrophobic sponge, and after the super-hydrophobic sponge is subjected to cyclic friction on the surface of sandpaper (600 meshes) for 40 times within a distance of 15cm, the contact angle of the super-hydrophobic sponge to water is more than 150 degrees, and the super-hydrophobic sponge has the characteristic of mechanical friction resistance.
Claims (16)
1. A method for preparing a micro-nano super-hydrophobic coating comprises the following steps:
1) dissolving fluorinated polysiloxane in a solvent a to obtain a solution a;
2) adding a solvent b into the solution a obtained in the step 1) in a dropwise manner for phase separation to obtain a system, namely the micro-nano super-hydrophobic coating;
the solvent a is at least one selected from tetrahydrofuran, acetone, ethyl acetate and butanone;
the solvent b is at least one selected from methanol, ethanol, isopropanol, water, toluene, xylene, n-hexane and cyclohexane.
2. The method of claim 1, wherein: in the step 1), the fluorinated polysiloxane is a polysiloxane with a side chain containing fluorine atoms, and is specifically selected from at least one of polytrifluoropropylmethylsiloxane, polymethylnonafluorohexylsiloxane, polytridecylfluorooctylmethylsiloxane and polymethylheptadecafluorodecylsiloxane;
wherein the weight average molecular weight of the polytrifluoropropylmethylsiloxane is 3000-100 ten thousand;
the weight-average molecular weight of the poly-methyl nonafluorohexylsiloxane is 4000-200 ten thousand;
the weight average molecular weight of the polytridecylfluorooctylmethylsiloxane is 5000-250 ten thousand;
the weight average molecular weight of the polymethylheptadecafluorodecylsiloxane is 6000-300 ten thousand;
the dissolving mode is stirring and dissolving; the stirring speed is 100-3000rpm, specifically 800-1000 rpm; stirring for 1-30 days, specifically 5 days;
in the solution a, the concentration of the fluorinated polysiloxane is 0.1-200mg/ml, preferably 25-50 mg/ml;
in the step 2), the mass ratio of the fluorinated polysiloxane to the solvent b is 1: 10-10000, preferably 1: 20-600;
in the dripping step, the dripping speed is 1 to 10 drops in 1 second;
the phase separation mode is stirring; the stirring speed is 100-3000rpm, specifically 500-1000 rpm.
3. A micro-nano scale superhydrophobic coating prepared by the method of any of claims 1-2.
4. The micro-nano scale superhydrophobic coating of claim 3, wherein: in the micro-nano super-hydrophobic coating, the particle size of the aggregate is 20 mu m-20 nm.
5. A method for preparing a nanoscale superhydrophobic coating, comprising the steps of: centrifuging the micro-nano scale superhydrophobic coating of any one of claims 3 or 4, and collecting a supernatant obtained after the centrifugation to obtain the nano scale superhydrophobic coating.
6. The method of claim 5, wherein: in the centrifugation step, the centrifugation rotating speed is 500rpm-12000rpm, the centrifugation time is 5min-30min, and the centrifugation radius is 6-12 cm.
7. The nanoscale superhydrophobic coating prepared by the method of claim 5 or 6.
8. The nanoscale superhydrophobic coating of claim 7, wherein: in the nanoscale superhydrophobic coating, the particle size of the aggregate is 20nm-100 nm.
9. Use of the micro-nanoscale superhydrophobic coating of claim 3 or 4 or the nanoscale superhydrophobic coating of claim 7 or 8 for the preparation of a superhydrophobic article;
alternatively, the use of the nanoscale superhydrophobic coating of claim 7 or 8 in the preparation of a superhydrophobic filter membrane;
or, a superhydrophobic article prepared from the micro-nanoscale superhydrophobic coating of claim 3 or 4 or the nanoscale superhydrophobic coating of claim 7 or 8;
or, the super-hydrophobic filter membrane prepared by the nano-scale super-hydrophobic coating of claim 7 or 8;
wherein the pore diameter of the super-hydrophobic product is 1-1000 μm;
the aperture of the super-hydrophobic filter membrane is 20nm-900 nm.
10. A method of making a superhydrophobic article comprising the steps of:
dipping or spraying the micro-nano scale superhydrophobic coating of claim 3 or 4 on a substrate, and drying to obtain the superhydrophobic article.
11. The method of claim 10, wherein: the material for forming the substrate is fiber or porous material, specifically fabric, sponge, metal filter screen or filter paper; the fabric is a natural textile or an artificial textile, and the natural textile is a cotton, hemp, silk or wool textile; the artificial textile is a terylene, polypropylene, chinlon, spandex or acrylic textile; the sponge is polyester, polyvinyl alcohol foaming sponge or polyether sponge; the metal filter screen is a stainless steel screen with the average aperture of 30-1000 μm; the filter paper is qualitative filter paper or quantitative filter paper;
in the drying step, the temperature is 25-100 ℃ and the time is 1-24 h.
12. A method for preparing a superhydrophobic filter membrane, comprising the steps of:
coating the nanoscale superhydrophobic coating of claim 7 or 8 on a filter membrane under vacuum, and drying to obtain the superhydrophobic filter membrane.
13. The method of claim 12, wherein: the aperture of the filter membrane is 20nm-900 nm;
the filter membrane is a nylon membrane, a polytetrafluoroethylene membrane, a polyvinylidene fluoride membrane, a mixed fiber ester membrane, a glass fiber membrane, an aluminum oxide membrane, a polyamide membrane, a cellulose acetate membrane, a polysulfone membrane, a polyether sulfone membrane or a polyvinyl alcohol membrane;
in the vacuum condition, the vacuum degree is 0.02-0.1 MPa;
in the drying step, the temperature is 30-100 ℃ and the time is 1-24 h.
14. A superhydrophobic article prepared according to claim 10 or 11; or,
the superhydrophobic filter membrane prepared according to claim 12 or 13.
15. The superhydrophobic article of claim 14, wherein: the superhydrophobic article is a superhydrophobic article having at least one of the following properties: solvent resistance, acid and alkali resistance, high temperature resistance and mechanical friction resistance;
wherein the high temperature resistance is the highest temperature resistance of 400 ℃.
16. Use of the superhydrophobic article or superhydrophobic filter membrane of claim 14 or 15 in oil-water separation.
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